摘要
目的:研究滇重楼药材中无机元素与有效成分的相关性。方法:采用高效液相色谱法(HPLC)测定药材中重楼皂苷Ⅰ、Ⅱ、Ⅵ、Ⅶ的含量:色谱柱为Phenomenex C18,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,检测波长为203 nm,柱温为30℃。采用电感耦合等离子体质谱法(ICP-MS)测定药材中钠(Na)、镁(Mg)、钾(K)、钙(Ca)、铬(Cr)、锰(Mn)、铁(Fe)、镍(Ni)、锌(Zn)、硒(Se)、锶(Sr)、钼(Mo)、铅(Pb)、镉(Cd)、汞(Hg)、铜(Cu)、砷(As)的含量:射频功率为1.55 k W,采样深度为10 mm,等离子气体流量为15.0 ml/min,载气流速为0.86 L/min,雾化室温度为2℃,碰撞模式为He,载气流量为4.5 ml/min,测量点数/峰为6,数据采样模式为跳峰采集(重复采集3次)。所得数据采用SPSS 21.0软件进行逐步回归分析,以评价上述两者的相关性。结果:重楼皂苷Ⅰ、Ⅱ、Ⅵ、Ⅶ检测进样量线性范围分别为0.939~4.697μg(r=0.999 9)、1.124~5.620μg(r=0.999 6)、0.784~3.918μg(r=0.999 8)、0.976~4.880μg(r=0.999 9);精密度、稳定性、重复性试验的RSD〈2%;加样回收率分别为96.53%~100.71%(RSD=1.69%,n=6)、98.19%~99.55%(RSD=0.58%,n=6)、95.45%~100.83%(RSD=1.87%,n=6)、96.11%~102.01%(RSD=2.07%,n=6)。17种无机元素检测含量线性范围为0~195.984 3 mg/kg(r≥0.999 3);检测限≤65.201 ng/kg。重楼皂苷Ⅰ含量与Mg呈正相关,与Pb呈负相关;重楼皂苷Ⅱ含量与Cu呈正相关,与As呈负相关;重楼皂苷Ⅵ含量与Sr、Hg呈正相关,与Mn呈负相关;重楼皂苷Ⅶ含量与Na、Ni呈正相关,与As呈负相关;4种重楼皂苷总含量与Ni、Sr呈正相关,与Fe呈负相关。结论:滇重楼药材中无机元素含量与有效成分存在一定相关性。
OBJECTIVE:To study the correlation of inorganic elements and active ingredients in Paris polyphylla. METHODS:HPLC was adopted for contents determination of polyphyllinⅠ,Ⅱ,Ⅵ and Ⅶ:the column was Phenomenex C18 with mobile phase of acetonitrile-water(gradient elution)at a flow rate of 1.0 ml/min,detection wavelength was 203 nm,and column temperature was 30 ℃. ICP-MS was adopted for contents determination of Na,Mg,K,Ca,Cr,Mn,Fe,Ni,Zn,Se,Sr,Mo,Pb,Cd,Hg,Cu and As:RF power was 1.55 k W,sampling depth was 10 mm,the plasma gas flow was 15.0 ml/min,carrier gas flow rate was 0.86 L/min,spray chamber temperature was 2 ℃,helium collision mode was He,gas flow was 4.5 ml/min,measurement points/peak was 6,sampling mode was hopping peak collection(repeated 3 times). And SPSS 21.0 software was adopted for stepwise regression analysis of correlation between the two above-mentioned. RESULTS:The linear range was 0.939-4.697 μg(r=0.999 8)for polyphyllinⅠ,1.124-5.620 μg(r=0.999 6)polyphyllinⅡ,0.784-3.918 μg for polyphyllin Ⅵ,0.976-4.880 μg for polyphyllin Ⅶ.RSDs of precision,stability and reproducibility tests were lower than 2%,recoveries were 96.53%-100.71%(RSD=1.69%,n=6)for polyphyllinⅠ,98.19%-99.55%(RSD=0.58%,n=6)forⅡ,95.45%-100.83%(RSD=1.87%,n=6)for polyphyllin Ⅵ,96.11%-102.01%(RSD=2.07%,n=6)for polyphyllin Ⅶ. The linear range was 0-195.984 3 mg/kg(r≥0.999 3),detection limit was no higher than 65.201 ng/kg. PolyphyllinⅠshowed positive correlation with Mg and negative correlation with Pb;polyphyllin Ⅱ showed positive correlation with Cu and negative correlation with As;polyphyllin Ⅵ showed positive correlation with Sr and Hg and negative correlation with Mn;polyphyllin Ⅶ showed positive correlation with Na and Ni and negative correlation with As;the total contents of the 4 polyphyllins showed positive correlation with Ni and Sr and negative correlation with Fe. CONCLUSIONS:The contents of inorganic elements and P. polyphylla have certain correlation with active ingredient.
出处
《中国药房》
CAS
北大核心
2016年第21期2951-2956,共6页
China Pharmacy
基金
国家自然科学基金资助项目(No.81260622)
贵州省科学技术厅科学技术基金资助项目(No.黔科合J字LKA〔2012〕07号)
贵州省大学生创新创业训练计划项目(No.201410067004)
安顺学院校级科研平台项目(No.2015AQ11)